WO2017009498A2 - Procédé pour la production d'urée organique, et urée organique et aus32 obtenus selon ce procédé - Google Patents

Procédé pour la production d'urée organique, et urée organique et aus32 obtenus selon ce procédé Download PDF

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Publication number
WO2017009498A2
WO2017009498A2 PCT/ES2016/000093 ES2016000093W WO2017009498A2 WO 2017009498 A2 WO2017009498 A2 WO 2017009498A2 ES 2016000093 W ES2016000093 W ES 2016000093W WO 2017009498 A2 WO2017009498 A2 WO 2017009498A2
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WO
WIPO (PCT)
Prior art keywords
urea
ammonia
stage
biomass
organic
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Ceased
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PCT/ES2016/000093
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English (en)
Spanish (es)
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WO2017009498A3 (fr
Inventor
Roberto ESTEFANO LAGARRIGUE
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Priority to US15/742,587 priority Critical patent/US20180208551A1/en
Priority to CN201680048493.3A priority patent/CN108064221A/zh
Priority to EP16823920.0A priority patent/EP3321251A2/fr
Publication of WO2017009498A2 publication Critical patent/WO2017009498A2/fr
Publication of WO2017009498A3 publication Critical patent/WO2017009498A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
    • C07C273/02—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds
    • C07C273/04—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds from carbon dioxide and ammonia
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C9/00—Fertilisers containing urea or urea compounds
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
    • C12M21/00—Bioreactors or fermenters specially adapted for specific uses
    • C12M21/04—Bioreactors or fermenters specially adapted for specific uses for producing gas, e.g. biogas
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00162—Controlling or regulating processes controlling the pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00164—Controlling or regulating processes controlling the flow
    • B01J2219/00166—Controlling or regulating processes controlling the flow controlling the residence time inside the reactor vessel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/18—Details relating to the spatial orientation of the reactor
    • B01J2219/185—Details relating to the spatial orientation of the reactor vertical
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel

Definitions

  • the invention refers to a process for the production of organic urea as well as organic urea and AUS32 obtained by this process.
  • the object of the present invention focuses specifically on a process for the production of organic urea which, in an innovative way, is carried out from biomass as a raw material, specifically, from the ammonia (NH 3 ) of biomass of plant and animal origin, mixing it with the recycled carbon dioxide (CO 2 ) from the exhaust gases of a combined cycle (gas - solids) bio-gas boiler with plant biomass, to form an intermediate compound, which is the that will produce organic urea.
  • NH 3 ammonia
  • CO 2 recycled carbon dioxide
  • urea is a colorless and crystalline chemical compound of formula C ⁇ ( ⁇ 2 ) 2. It is found abundantly in the urine and in the stool. It is the main terminal product of protein metabolism in man and other mammals. Human urine contains about 20g per liter. In smaller quantities, it is present in the blood, in the liver, in the lymph and in the serous fluids and also in the excrements of fish and many other animals. It is also found in the heart, in the lungs, bones, in the reproductive organs (semen), fungi, legumes and cereals.
  • Urea currently serves as a raw material for the formation of livestock feed, agricultural fertilizers, moisturizers and as AUS32 (AdBlue ®) which is a chemical reactor for the degradation of nitrous oxide in the exhaust gases generated basically by engines Internal combustion Obtaining said compound at the industrial level will be conditioned by the formation of carbomatos, in any of its raw materials (Biomass and / or Hydrocarbon Gas)
  • urea and phosphate fertilizers allows plantations to become stronger and can cope, with the help of the necessary agrochemicals, different types of insects, bacteria and viruses that could affect you during the time of maturation of its fruits
  • urea within systems operating with SCR (Selective Catalytic Reduction) as the main component in the chemical reactor AUS32 (AdBlue ®) (urea and distilled water) allows a significant decrease in the emissions generated by the gases of Exhaust of internal combustion engines, mobile and stationary.
  • SCR Selective Catalytic Reduction
  • AUS32 AdBlue ®
  • Organic urea also known as carbamide, carbonyldiamide or arbamide acid, is the name of the carbonic acid in di amide, whose chemical formula is (NH2) 2CO.
  • CO 2 is obtained from natural gas, through the reaction known as reforming.
  • the impurities of the gas such as oil droplets, dust particles, and above all desulfurize the gas, must be separated, since sulfur interferes with the action of the catalysts.
  • CO 2 is obtained by means of two stages of catalytic reforming with water vapor.
  • the heat necessary for the reaction comes from the combustion of natural gas and partially reformed gases. Air is allowed to enter the reactor to obtain the necessary H2 / N2 ratio for the subsequent obtaining of ammonia.
  • the reaction is as follows; The two stages of reforming are verified according to the reaction described, and at the exit of the second stage, a gas is obtained with the following proportions: 56% Ha, 12% CO, 8% CO 2 , 23% N2 and less than 0 , 5% CH4.
  • the conversion of CO is carried out by causing it to react catalytically with water vapor to form CO 2 and H2 using iron and copper as catalysts.
  • the circulating gas is composed of air, methane and water vapor, which react with an iron catalyst to form ammonia in a gaseous state according to: 7 CH4 + 10 H2O + 8 N2 + 2 O2 16 NH3 + 7 CO 2
  • the gaseous ammonia condenses on cooling and separates from the gas to store it under pressure of about 13 atmospheres.
  • the remaining gaseous ammonia is recirculated to the synthesis loop.
  • CO 2 Before entering the reactor, CO 2 is compressed up to 200 atm, using an electric compressor and ammonia up to 145 atm,
  • the molten urea is pumped to the top of the tower 80 meters high and 16 meters in diameter. Through a rotating basket with about 8000 Small perforations are able to obtain a molten Urea rain, whose droplets are solidified first and then cooled during their free heat, while air is circulated in the opposite direction by means of large fans located at the top of the tower.
  • the mixed components form the ammonium carbomate
  • the ammonium carbomate dehydrates to form urea.
  • the reaction rates are different.
  • the first stage is much faster than the second stage, whereby intermediate carbomate accumulates.
  • the first reaction is not fully verified, so there is also free ammonia and dioxide.
  • carbomate is a highly corrosive product, therefore, what is done is to degrade the part of carbomate not converted to urea into its reagents of origin, and then re-form it.
  • the first reaction is exothermic
  • the second is endothermic
  • ⁇ animal such as excrements (purines) from pigs, poultry, cattle, wool, the blood of these animals, the coatings or the organic components thereof such as viscera, or
  • Vegetable such as Mediterranean pineapple, tree and shrub leaves, vegetables, fruits, or other forest-derived components such as barks or pine nuts.
  • C02 carbon dioxide
  • the raw materials involved in the production of hydrocarbon-based urea are: the “Ammonia” (NHb) from the cracking of the "reformed gas” (cracking-breaking of the molecules of CH 4 ) (Hydrocarbons) and the dioxide carbon (CO 2) from natural gas, by the reaction known as reforming. Combined these two elements urea is produced.
  • the process for the production of organic biomass-based urea, object of the present invention comprises the following stages: - Methane stage: The first thing is to load a compound consisting of: "into a biomass” digester ":” pig purines, pig blood, chicken purines, chicken blood, pinnace leaves, pinnace ashes and water "or any of the other plant / animal / human biomass described above. This mixture is externally heated to accelerate and produce a chemical reaction that allows to obtain methane gas, air, ammonia in the gaseous state and water vapor and PH regulator.
  • - Catalyst stage The mass of gases obtained in the previous stage is condensed by cooling and the gaseous ammonia is separated for storage at a pressure of 13 atmospheres. The remaining gaseous ammonia is recirculated to the synthesis loop.
  • - Carbony formation stage The Urea synthesis reaction is carried out at high pressures (200 bar) and the optimum thermal level (190 ° C) in a special stainless steel reactor.
  • Ammonium carbomate is produced between CO 2 and NH 3 causing an exothermic reaction.
  • Conversion is in the order of 70%. That is, of every 100 kg of carbomate that is formed, only 70 kg become urea. The rest is You must permanently recycle continuously to achieve total conversion.
  • Said degradation is preferably carried out, as it is more economical, through stripping (detachment) of the ammonia, displacing the reaction towards the products that form it.
  • stripping detachment
  • the system reacts towards equilibrium by degrading carbomate.
  • Urea production is achieved in a vertical reactor, which operates at 188
  • One of the options to optimize the process is to perform combined operations for carbomate formation (exothermic and rapid) in the lower part of said reactor by feeding excess CO 2 and NH 3 and decomposing carbonate in urea (much slower and endothermic).
  • Biuret is formed when two urea molecules bind releasing an ammonia molecule: It is a highly toxic substance for plants and inconvenient for its use in products to reduce emissions of nitrogen oxides, such as the chemical reactor AUS32 (AdBlue®). To lower its concentration in values below 0.35%, it must be achieved an excess of ammonia in the synthesis of urea (therefore preferably, the combined biomass of animals and vegetables are used.) This can be achieved by a vacuum concentrator which is heated (by applying external heat) using the residual water vapor of the steam generator This method is called synthesis urea which, once achieved, is pumped to an evaporation unit.
  • urea has multiple applications and uses, so it is an interesting product and of great possibilities for its industrial production, although, in the case of organic biomass urea, the possibilities of use and advantages are much greater.
  • urea Due to its high nitrogen content, commercially prepared urea is used in the manufacture of agricultural fertilizers, as a stabilizer in carbon-cellulose explosives or as a basic component of synthetically prepared resins. It is also used in feed for ruminants as a food supplement. In dermatology it is also used as a natural moisturizer. It is present in adhesives, plastics, resins, inks, pharmaceuticals and finishes for textiles, paper and metals.
  • fertilizers are critical to achieve the level of agricultural production necessary to feed the rapidly growing world population.
  • the organic biomass urea production process allows multiple actions to be carried out in said factories such as:
  • Methane gas electric generator
  • organic biomass urea organic biomass urea
  • the procedure is a great advantage in terms of providing indirect positive impacts to the natural environment that come from the proper use of plant and animal biomass;
  • manufacture of fertilizers on an organic basis that allow intensifying agriculture on existing lands, reducing the need to expand it to other lands that may have different natural or social uses. It is also reduced substantially !
  • the negative environmental impacts of hydrocarbon-based fertilizer production are often severe. Wastewater is not a problem. Having been treated as part of the process they are slightly acidic (depending on the type of plant), and their toxic substance content is minimal (concentrations of: ammonia or the compounds of ammonium, urea, cadmium, arsenic, fluorides and phosphate).
  • the treatment of water as an active agent in the manufacture of organic urea is the cause of its effluents, total suspended solids, nitrate and organic nitrogen, phosphorus, potassium, and (as a result), being within the normal parameters for fertigation in BOD (biological oxygen demand) and COD (chemical oxygen demand).
  • BOD biological oxygen demand
  • COD chemical oxygen demand
  • Figure 1 Shows, by means of a block diagram, an outline of the steps of the process for the production of organic urea, object of the invention. PREFERRED EMBODIMENT OF THE INVENTION
  • - Methane stage (1) that in an "digester” of biomass, animal and vegetable biomass are mixed (2) formed by: "pig purines, pig blood, chicken purines, chicken blood, pinnace leaves, ashes of pinnace and water "that is heated externally to obtain: methane gas, air, ammonia in the gaseous state and water vapor and PH regulator.
  • - Catalyst stage (3) where the mass of gases obtained in the previous stage is condensed by cooling and the gaseous ammonia is separated for storage at a pressure of 13 atmospheres. The remaining gaseous ammonia (4) is recirculated to the synthesis loop.
  • Carbonate formation stage (5) where the Urea synthesis reaction is carried out at high pressures (200 bar) and the optimum thermal level (190 ° C) in a special stainless steel reactor.
  • Ammonium carbomate is produced between CO 2 and NH 3 producing an exothermic reaction.
  • Urea production is achieved in a vertical reactor, which operates at 188
  • One of the options to optimize the process is to carry out combined operations for the formation of carbomate (exothermic and rapid) in the lower part of said reactor through the supply of excess CO 2 and NH 3 and the decomposition of carbomate in urea (much slower and endothermic).
  • This stage is essential to reduce the biuret, having to reach a concentration of 80% urea.
  • - Evaporation Stage (9) The current from the concentrator is still concentrated in two stages of evaporation, the first one (concentrates up to 95%) operating at absolute 0.3 kg / cm2 and the second (concentrates up to 99.8%) at very high vacuum, to achieve evaporation of water without thermally decomposing urea. A large ejector must be used to achieve the required vacuum levels.
  • This urea obtained with the process of the invention has been manufactured from biomass as well as the chemical reactor AUS32 (AdB ⁇ ue®) comprises the urea manufactured according to the invention.
  • a granulation stage (10) is contemplated where the current can be sent to a Prilling Tower or granulation, for the formation of urea beads.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Wood Science & Technology (AREA)
  • Molecular Biology (AREA)
  • Zoology (AREA)
  • Genetics & Genomics (AREA)
  • Sustainable Development (AREA)
  • Biomedical Technology (AREA)
  • Biotechnology (AREA)
  • Microbiology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Biochemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Fertilizers (AREA)

Abstract

L'invention concerne un procédé de production d'urée organique qui est préparée à partir du mélange et de la réaction entre l'ammoniac (NH3) liquide et l'anhydride carbonique (CO2) gazeux lors d'étapes de formation de carbomate (5) d'ammonium, de décomposition du carbomate (7), de synthèse de l'urée (8) et d'évaporation (9) de celle-ci. Le procédé est mis en oeuvre à partir d'ammoniac organique de biomasse (2) animale et végétale et de dioxyde de carbone recyclé de gaz (6) de chaudières biogaz à biomasse végétale, comprenant des étapes préalables de méthanation (1), avec un "digesteur" de biomasses mélangeant des purins et du sang de porc et de poulet, des feuilles et des cendres de pin, et de l'eau, jusqu'à obtenir du gaz méthane, de l'air, de l'ammoniac à l'état gazeux et de la vapeur d'eau et un régulateur de pH et de catalysation (3), les gaz obtenus étant condensés par refroidissement et l'ammoniac gazeux étant séparé pour le stocker à 13 atmosphères. L'invention concerne également l'urée organique et le réacteur chimique AUS32 (AdBlue®) fabriqué à partir de la biomasse.
PCT/ES2016/000093 2015-07-08 2016-09-08 Procédé pour la production d'urée organique, et urée organique et aus32 obtenus selon ce procédé Ceased WO2017009498A2 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
US15/742,587 US20180208551A1 (en) 2015-07-08 2016-09-08 Method for producing organic urea and the organic urea and aus32 thereby obtained
CN201680048493.3A CN108064221A (zh) 2015-07-08 2016-09-08 用于生产有机尿素的方法和由其获得的有机尿素及aus32
EP16823920.0A EP3321251A2 (fr) 2015-07-08 2016-09-08 Procédé pour la production d'urée organique, et urée organique et aus32 obtenus selon ce procédé

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ES201530983A ES2573717B1 (es) 2015-07-08 2015-07-08 Procedimiento para la producción de urea orgánica así como urea orgánica y AUS32 obtenidas por este procedimiento
ESP201530983 2015-07-08

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WO2017009498A2 true WO2017009498A2 (fr) 2017-01-19
WO2017009498A3 WO2017009498A3 (fr) 2017-05-11

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PCT/ES2016/000093 Ceased WO2017009498A2 (fr) 2015-07-08 2016-09-08 Procédé pour la production d'urée organique, et urée organique et aus32 obtenus selon ce procédé

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US (1) US20180208551A1 (fr)
EP (1) EP3321251A2 (fr)
CN (1) CN108064221A (fr)
ES (1) ES2573717B1 (fr)
WO (1) WO2017009498A2 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019115044A1 (fr) * 2017-12-14 2019-06-20 FRIEDMAN, Michael John Procédé de liaison d'ammoniac agricole dangereux à l'aide de dioxyde de carbone organique

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EP3398935A1 (fr) * 2017-05-05 2018-11-07 Casale Sa Procédé et installation de synthèse de l'urée
CN109665976B (zh) * 2018-11-15 2021-10-19 锦西天然气化工有限责任公司 一种氨法回收烟道气co2与尿素联合生产的工艺
FI129441B (en) * 2019-11-20 2022-02-28 Andritz Oy Method for producing cellulose carbamate
US20240059575A1 (en) * 2022-08-09 2024-02-22 Circular Upcycling Method of Bioammonia Production from Wastewater Through Application of Mass-Transfer Reaction Kinetics
LU103016B1 (de) 2022-09-23 2024-03-25 Thyssenkrupp Ind Solutions Ag Verfahren zur Herstellung von grünem Harnstoff
EP4590420A1 (fr) 2022-09-23 2025-07-30 thyssenkrupp Uhde GmbH Système et procédé de production d'urée verte
DE102022210054A1 (de) 2022-09-23 2024-03-28 Thyssenkrupp Ag Verfahren zur Herstellung von grünem Harnstoff
LU103015B1 (de) 2022-09-23 2024-03-25 Thyssenkrupp Ag Anlage und Verfahren zur Erzeugung von grünem Harnstoff
DE102023115887A1 (de) 2023-06-16 2024-12-19 Christian Nissing Verfahren zur herstellung von harnstoff auf basis von erneuerbaren energieträgern
DE102023003422A1 (de) 2023-08-19 2025-02-20 Horst Bendix Verfahren zur Herstellung von Ammoniak und Harnstoff aus Bio-Ethanol
CN120233747B (zh) * 2025-05-29 2025-08-19 杨凌霖科生态科技股份有限公司 肥料生产能耗实时优化方法

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US6976362B2 (en) * 2001-09-25 2005-12-20 Rentech, Inc. Integrated Fischer-Tropsch and power production plant with low CO2 emissions
EP1928984A1 (fr) * 2005-08-19 2008-06-11 Varipower Technology PTY Ltd Methode de generation de puissance
US20080040975A1 (en) * 2006-08-21 2008-02-21 Albert Calderon Method for maximizing the value of carbonaceous material
US9352329B2 (en) * 2008-08-12 2016-05-31 4A Technologies, Llc Modularized system and method for urea production using a bio-mass feedstock
AU2010256286B2 (en) * 2009-06-05 2016-01-28 Industrial Ecosystems Pty Ltd Method and integrated system for producing electric power and fertiliser

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019115044A1 (fr) * 2017-12-14 2019-06-20 FRIEDMAN, Michael John Procédé de liaison d'ammoniac agricole dangereux à l'aide de dioxyde de carbone organique

Also Published As

Publication number Publication date
WO2017009498A3 (fr) 2017-05-11
CN108064221A (zh) 2018-05-22
ES2573717B1 (es) 2017-01-16
ES2573717A1 (es) 2016-06-09
EP3321251A2 (fr) 2018-05-16
US20180208551A1 (en) 2018-07-26

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